WO2011106879A1 - Système d'extraction à l'organosolv par lots multiples - Google Patents

Système d'extraction à l'organosolv par lots multiples Download PDF

Info

Publication number
WO2011106879A1
WO2011106879A1 PCT/CA2011/000227 CA2011000227W WO2011106879A1 WO 2011106879 A1 WO2011106879 A1 WO 2011106879A1 CA 2011000227 W CA2011000227 W CA 2011000227W WO 2011106879 A1 WO2011106879 A1 WO 2011106879A1
Authority
WO
WIPO (PCT)
Prior art keywords
solvent
extraction
primary
accumulator
extractor
Prior art date
Application number
PCT/CA2011/000227
Other languages
English (en)
Inventor
Paul Kenneth Adam
Stephan Richard Winner
Original Assignee
Lignol Innovations Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lignol Innovations Ltd. filed Critical Lignol Innovations Ltd.
Publication of WO2011106879A1 publication Critical patent/WO2011106879A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G1/00—Lignin; Lignin derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B01D11/0284—Multistage extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00—Macromolecular compounds derived from lignocellulosic materials

Definitions

  • This invention relates to systems and processes for batch organosolv extraction of lignin and other species from biomass feedstocks. More particularly, this invention relates to improved configurations of the extraction system.
  • the various chemical components within typical biomass can be employed in a variety of ways.
  • the cellulose in plant matter may desirably be separated out and fermented into fuel grade alcohol.
  • the lignin component which makes up a significant fraction of species such as trees and agricultural waste, has huge potential as a useful source of phenol containing chemicals for numerous industrial applications.
  • most separation techniques employed by industry today are too aggressive and chemically alter the lignin component during separation to the point where it is no longer acceptable for use in most of these potential applications.
  • Organosolv extraction processes are typically less aggressive and can be used to separate lignin and other useful materials from biomass without unacceptably altering or damaging the lignin. Such processes can therefore be used to maximize the value from all the components making up the biomass. Organosolv extraction processes however typically involve extraction at higher temperatures and pressures with a flammable solvent than other industrial methods and thus are generally more complex and expensive. While large scale commercial viability had been demonstrated decades ago from a technical and operation perspective, organosolv extraction has not, to date, been considered economical.
  • Fig. 1 depicts the important components in the organosolv extraction system.
  • a supply of appropriate biomass e.g. wood chips
  • the first extraction solution employed is a twice-used "primary solvent” (from previous biomass batches) obtained from primary solvent accumulator 3.
  • Lignin and other materials are then extracted from the biomass into the primary solvent and the resulting "black liquor” is displaced into recovery feed accumulator 5.
  • the second extraction solution is a once-used "secondary solvent” (from a previous biomass batch) obtained from secondary solvent accumulator 6.
  • the third extraction solution is a fresh ethanol/water mixture obtained from fresh solvent accumulator 7. Again, material is extracted from the biomass and the resulting liquor is displaced into secondary solvent accumulator 6.
  • a typical multiple batch organosolv extraction system may simply be configured as a parallel array of systems like those depicted in Fig. 1. Such a configuration is implied in the paper "The ALCELLTM process - A proven alternative to Kraft pulping", Pye and Lora, Tappi Journal, March 1991 , Vol. 74(3) in which the illustrated system comprises multiple extractors with each expected to require its own set of accumulators but perhaps with a common recovery accumulator and a fresh solvent supply.
  • biomass processed in the organosolv extraction system undergoes a primary solvent extraction followed by a secondary solvent extraction.
  • the solvent used for the primary solvent extraction is generally the liquor obtained from the secondary solvent extraction.
  • the system comprises at least one, usually two or more, extractor, a number of primary accumulators, and a supply of fresh solvent.
  • the number of primary accumulators is fewer than the number of extractors and at least one of the primary accumulators is fluidly connected to more than one extractor.
  • the fresh solvent can be an aqueous mixture of ethanol and water and can be used to extract lignin and other desirable co-products from the biomass.
  • the process can be a two stage process (e.g. where the solvent used for the secondary solvent extraction is fresh solvent) and a fresh solvent accumulator may be incorporated for temporary storage of fresh solvent from the fresh solvent supply.
  • the fresh solvent accumulator may supply more than one extractor and thus can be fluidly connected to more than one extractor.
  • the process can be a three stage process (e.g. as in the aforementioned US4764596) in which the secondary solvent extraction is followed by a tertiary solvent extraction, and in which the solvent used for the secondary solvent extraction is the liquor obtained from the tertiary solvent extraction and the solvent used for the tertiary solvent extraction is fresh solvent.
  • a secondary accumulator may additionally be included for temporary storage of drain liquor from the tertiary solvent extraction.
  • the secondary accumulator may be fluidly connected to more than one extractor.
  • a preferred system can comprise six extractors wherein the first, fourth and fifth extractors are fluidly interconnected and wherein the second, third and sixth extractors are fluidly interconnected, three primary accumulators wherein the first, second, and third primary accumulators are fluidly connected to the first and second extractors, the third and fourth extractors, and the fifth and sixth extractors respectively, and a fresh solvent accumulator fluidly connected to each of the extractors and to the fresh solvent supply.
  • the system can comprise a recovery accumulator that is optionally fluidly connected to each of the extractors.
  • the system can comprise a lignin recovery subsystem comprising one or more flash tanks and other conventional components.
  • the flash tank/s is/are fluidly connected to the recovery accumulator and may be arranged in series.
  • the process in general may comprise: a) extracting material from the biomass in a first extractor using primary extraction solvent obtained from a primary accumulator; b) removing the liquor from the primary solvent extraction in the first extractor;
  • the liquors in steps b) and d) may be delivered to a flash tank fluidly connected to the first and second extractors.
  • these liquors may be directed to a recovery accumulator fluidly connected between the first and second extractors and the flash tank.
  • the process can comprise:
  • the duration of the primary solvent extraction may be an integer multiple of the duration of the secondary solvent extraction (which, in a two stage process, is the duration of the fresh solvent extraction). For instance, in some embodiments, the duration of the primary solvent extraction can be about an hour. In a two or three stage process then, the duration of the secondary and tertiary solvent extraction times can both be about half an hour. In such a situation, the residence time for liquor in the recovery accumulator can be kept desirably brief, i.e. less than about an hour.
  • Fig. 1 shows a schematic of a prior art system having a single extractor, a single primary accumulator, and a secondary accumulator and a tertiary (fresh solvent) accumulator.
  • Fig. 2 shows a partial schematic of an embodiment of the invention employing 6 extractors (1-6), 3 primary accumulators (11-13) and 1 tertiary (fresh solvent) accumulator (21) (only the portion showing these elements is shown).
  • Fig. 3 shows a partial schematic of another embodiment of the invention employing 7 extractors (1-7), 4 primary accumulators (11-14), and 1 secondary accumulator (31) (only the portion showing these elements is shown).
  • Fig. 4 shows a partial schematic of another embodiment of the invention employing 7 extractors (1-7), 4 primary accumulators (11-14), and 1 tertiary (fresh solvent) accumulator (21) (only the portion showing these elements is shown).
  • At least one primary accumulator may be shared by at least two extractors.
  • some primary accumulators can be eliminated.
  • other accumulators in the system may be shared and/or completely eliminated (e.g. secondary accumulators, recovery accumulators, tertiary accumulators where applicable). For instance, it may be possible to direct the liquor from one extraction stage and coming from one extractor, directly to another extractor to serve as solvent for an earlier extraction stage. In this way, no accumulator is needed for the earlier extraction stage.
  • sharing is possible if there are a sufficient number of extractors in the system and if the duration and relative timing of the various steps in the process sequence are adjusted appropriately.
  • sharing can be accomplished if the start and end times of key steps in the individual extraction sequence can be matched appropriately amongst the various extractors in the system.
  • the duration of the primary extraction step can desirably be an integer multiple of the secondary and/or tertiary extraction steps.
  • the primary extraction step generally lasts as long or longer than subsequent extraction steps and can be of the order of 1 -2 hours in duration.
  • the multiple batch, multiple extractor system and process are suitable for the organosolv extraction of lignin from lignocellulosic feedstocks using an aqueous ethanol solvent mixture.
  • organosolv extraction of lignin from lignocellulosic feedstocks using an aqueous ethanol solvent mixture are illustrated in the Examples below. And more specifics for adjusting step duration and for matching the start and end of the various steps should be easily understood by way of reference to these detailed Examples. Those skilled in the art will readily appreciate that many other configurations and timings may be possible within the allowable constraints for any given specific situation.
  • the processes provided herein comprise the displacement of one liquor with another.
  • the primary liquor is replaced by the secondary liquor.
  • one liquor is displaced by the additional of the replacement liquor i.e. as the secondary liquor enters the primary extractor it displaces the primary liquor.
  • the displacing liquor is added from the top or the extraction vessel and that the displaced liquor is removed from the bottom.
  • this configuration offers advantages over the established process. For example, a higher yield of lignin may be extracted from the biomass. Additionally, this may allow for using an extractor for feeding a pump and therefore eliminate the need for an accumulator.
  • FIG. 2 A preferred configuration for a commercial organosolv extraction system is shown in the partial schematic of Figure 2. For simplicity, only the portion comprising the multiple extractors and accumulators involved in solvent extraction are shown. The rest of the system is similar to that shown in Figure 1.
  • the system of Figure 2 is designed for a three stage extraction of biomass and employs 6 biomass extractors (1-6), three primary accumulators (11-13), a recovery accumulator (not shown), no secondary accumulators, and one common tertiary fresh solvent accumulator (21).
  • the top headers of the extractors are fluidly interconnected via suitable piping and valving.
  • the bottom headers of extractors are also fluidly interconnected together.
  • the primary accumulators are denoted 1 1, 12, and 13 respectively.
  • each pair of extractors shares a common primary accumulator.
  • Appropriate plumbing is provided such that each primary accumulator can fill from each extractor in its associated pair and also such that each extractor in a pair can be filled by its associated primary accumulator.
  • tertiary fresh solvent accumulator 21 is provided to temporarily hold fresh solvent for purposes of supplying fresh solvent to each of the six extractors for the tertiary fresh solvent extraction stage (i.e. accumulator 21 is shared amongst all the extractors). Appropriate fluid connections are therefore provided from fresh solvent accumulator 21 to each extractor 1, 2, 3, 4, 5, and 6.
  • Table 1 shows a potentially suitable, practical timing sequence over a complete cycle for this multiple extractor system.
  • the sequence is to first fill an extractor with biomass chips (denoted "chip fill” in Table 1).
  • Next steam is introduced to pre-heat the biomass ("pre- steam") and is continued until sufficient oxygen is removed to reduce the risk of combustion and to permit safe operation.
  • pre- steam is introduced to pre-heat the biomass
  • hold a hold period after the pre-steam
  • primary extraction solvent from a primary accumulator is flash filled into the extractor and heated to the target extraction temperature (“flash fill & heat-up").
  • the duration of this step is 1 hour, there are 6 extractors undergoing this step in series (i.e. one extractor is always undergoing this step over the 6 hour period), and the overall cycle time of the system is 6 hours, this arrangement desirably results in a leveling out of the heating requirements for the overall system.
  • the primary solvent extraction then is allowed to take place over about a 60 minute period. Towards the end of this period, typically 10-15 minutes before the end, some of the liquor is removed and sent to the recovery accumulator.
  • Table 1 shows the timing sequences for all the extractors, the primary accumulators, and the common tertiary fresh solvent accumulator in the system shown. Table 1 also shows the timing sequence for the common recovery accumulator. Here, a complete cycle takes 6 hours and each cycle is 1 hour out of phase with the next.
  • FIG. 3 shows an alternative embodiment for a commercial organosolv extraction system. Again, only the portion comprising the multiple extractors and accumulators involved in solvent extraction are shown. The rest of the system is similar to that shown in Figure 1.
  • the system in Figure 3 is also designed for a three stage extraction of biomass and employs seven biomass extractors (1-7), four primary accumulators (11-14), one secondary accumulator (31), and no tertiary fresh solvent accumulator.
  • Like numerals as those used in Figure 2 have been employed in Figure 3.
  • associated Table 2 shows a potentially suitable, practical timing sequence over a complete cycle for this multiple extractor system.
  • the duration of the primary extraction is also 1 hour but now 1 hour is also provided for the secondary and tertiary fresh solvent extraction steps.
  • a complete cycle takes 7 hours with a 1 hour delay in starting up.
  • FIG 4 shows yet another alternative embodiment for a commercial organosolv extraction system. Again, only the portion comprising the multiple extractors and accumulators involved in solvent extraction are shown. The rest of the system is similar to that shown in Figure 1.
  • the system in Figure 4 is also designed for a three stage extraction of biomass and employs seven biomass extractors (1-7), four primary accumulators (11-14), no secondary accumulator, and a common tertiary fresh solvent accumulator (21). (Note: although not apparent in the Figure, a fresh solvent accumulator is generally optional and here would be relatively small). Like numerals as those used in the previous Figures have been employed in Figure 3.
  • Example 2 With this arrangement, the advantages of Example 2 can still be generally obtained. However, secondary accumulator 31 can be eliminated at the expense of a modest increase in overall cycle time.
  • secondary accumulator 31 can be eliminated at the expense of a modest increase in overall cycle time.
  • the principles of the invention may be applied to a two-stage extraction process or an extraction process with three or more stages. Accordingly, the scope of the invention is to be construed in accordance with the substance defined by the following claims.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

L'extraction à l'organosolv de la lignine et autres matériaux contenus dans des charges d'origine biomassique selon l'invention peut être réalisée à l'aide d'une procédure d'extraction par lots multi-étage telle que le procédé ALCELL®. Pour plusieurs raisons, des infrastructures commerciales peuvent tirer profit du traitement de multiples lots simultanément à l'aide de multiples extracteurs et du matériel associé. Une modification appropriée des séquences de synchronisation et de la conception du système permet de partager, voire d'éliminer, bon nombre des accumulateurs de solvant typiquement utilisés dans ces systèmes et, par conséquent, de réduire le coût et de simplifier la conception du système.
PCT/CA2011/000227 2010-03-01 2011-03-01 Système d'extraction à l'organosolv par lots multiples WO2011106879A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA2695083A CA2695083A1 (fr) 2010-03-01 2010-03-01 Systeme d'extraction de substances organosolubles en lots multiples
CA2,695,083 2010-03-01

Publications (1)

Publication Number Publication Date
WO2011106879A1 true WO2011106879A1 (fr) 2011-09-09

Family

ID=44515256

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CA2011/000227 WO2011106879A1 (fr) 2010-03-01 2011-03-01 Système d'extraction à l'organosolv par lots multiples

Country Status (2)

Country Link
CA (1) CA2695083A1 (fr)
WO (1) WO2011106879A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9708490B2 (en) 2009-05-28 2017-07-18 Fibria Innovations Inc. Derivatives of native lignin
US9840621B2 (en) 2011-03-24 2017-12-12 Fibria Innovations Inc. Compositions comprising lignocellulosic biomass and organic solvent
US9982174B2 (en) 2010-02-15 2018-05-29 Fibria Innovations Inc. Binder compositions comprising lignin derivatives
US10533030B2 (en) 2010-02-15 2020-01-14 Suzano Canada Inc. Carbon fibre compositions comprising lignin derivatives
US11118017B2 (en) 2019-11-13 2021-09-14 American Process International LLC Process for the production of bioproducts from lignocellulosic material
US11306113B2 (en) 2019-11-13 2022-04-19 American Process International LLC Process for the production of cellulose, lignocellulosic sugars, lignosulfonate, and ethanol

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4100016A (en) * 1975-10-24 1978-07-11 C P Associates Limited Solvent pulping process
US4764596A (en) * 1985-11-05 1988-08-16 Repap Technologies Inc. Recovery of lignin
GB2439135A (en) * 2006-06-13 2007-12-19 Ecopulpa Limitada Pulp process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4100016A (en) * 1975-10-24 1978-07-11 C P Associates Limited Solvent pulping process
US4764596A (en) * 1985-11-05 1988-08-16 Repap Technologies Inc. Recovery of lignin
GB2439135A (en) * 2006-06-13 2007-12-19 Ecopulpa Limitada Pulp process

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PYE, E. K. ET AL.: "The AlcellTM process A proven alternative to kraft pulping", TAPPI JOURNAL, March 1991 (1991-03-01) *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9708490B2 (en) 2009-05-28 2017-07-18 Fibria Innovations Inc. Derivatives of native lignin
US10435562B2 (en) 2009-05-28 2019-10-08 Fibria Innovations Inc. Derivatives of native lignin, lignin-wax compositions, their preparation, and uses thereof
US9982174B2 (en) 2010-02-15 2018-05-29 Fibria Innovations Inc. Binder compositions comprising lignin derivatives
US10533030B2 (en) 2010-02-15 2020-01-14 Suzano Canada Inc. Carbon fibre compositions comprising lignin derivatives
US9840621B2 (en) 2011-03-24 2017-12-12 Fibria Innovations Inc. Compositions comprising lignocellulosic biomass and organic solvent
US11118017B2 (en) 2019-11-13 2021-09-14 American Process International LLC Process for the production of bioproducts from lignocellulosic material
US11306113B2 (en) 2019-11-13 2022-04-19 American Process International LLC Process for the production of cellulose, lignocellulosic sugars, lignosulfonate, and ethanol

Also Published As

Publication number Publication date
CA2695083A1 (fr) 2011-09-01

Similar Documents

Publication Publication Date Title
WO2011106879A1 (fr) Système d'extraction à l'organosolv par lots multiples
EP2075347B1 (fr) Procédé et système de saccharification hydrolytique d`une biomasse cellulosique
KR101390386B1 (ko) 바이오매스 성분을 분리하는 방법
US12037563B2 (en) Modular, mobile, and automated solvent extraction and distillation systems, and methods of using the same
EP2185734B1 (fr) Procédé et système pour le prétraitement d'une substance lignocellulosique
DE102009010233B4 (de) Verfahren zum Erzeugen von Kohle aus Biomasse
JP7411567B2 (ja) リグノセルロースのバイオマスの処理方法
AU2007324208B2 (en) A procedure and equipment thereof for comprehensive utilization of Radix pueraria
CN103403192A (zh) 用于生物质原料的通过在加压热水中进行处理的受控液化的工艺
EP3156539B1 (fr) Procédé de prétraitement continu d'une charge d'alimentation lignocellulosique
US1690954A (en) Process for the extraction of cellulose or paper pulp from fibrous vegetable matter containing the same
CN102000445B (zh) 亚临界连续萃取除虫菊生产工艺
CN104379768A (zh) 用于生物质的液化的两步优化
CN101608000A (zh) 一种木聚糖的连续蒸煮提取方法、设备及其应用
US20090114591A1 (en) System and Method for Pretreating Biomass
WO2020261291A1 (fr) Procédé de production d'éthanol à partir de fibres de maïs
CN107074602A (zh) 有机物质的连续热水解的方法及适合实施所述方法的体系
CN108383691B (zh) 一种从虎杖中提取白藜芦醇的方法
CN109836483B (zh) 玉米醇溶蛋白的生产装置和生产方法
CN105481872B (zh) 一种恒温梯度串联提取植物活性成分的方法
US20210253975A1 (en) Modular, mobile, and automated solvent extraction and distillation systems, and methods of using the same
CN106674540A (zh) 一种杜仲胶的制备方法
CN108358774A (zh) 利用渗透汽化-结晶耦合多重回收组分的方法和装置
CN106635389A (zh) 一种亚麻籽油的提取方法
Viola et al. Guayule stems fractionation and sugars recovery by different pretreatment technologies

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11750118

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 11750118

Country of ref document: EP

Kind code of ref document: A1